HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → HCID 20308023, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Lithium | HCID 3028194 | — |
| Reactant | HCID 20308034 | HCID 20308034 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 20308023 | HCID 20308023 | 79.2% |
Reaction Steps
A solution of 16.3 g of crude 1,2,3,4-tetrahydro-1-(piperidinomethyl)fluorene-2-methanol, in the form of the free base, dissolved in 300 ml of ether is added to 1.5 liter of liquid ammonia. An amount of 8.4 g (1.2 moles) of lithium ribbon is added over 1.5 hr. and then 150 ml of abs. ethanol added over 60 minutes; the ammonia is evaporated and the residue cooled and partitioned between 400 ml of water and 300 ml of ether. The aqueous layer is washed with 2 × 250 ml of ether, and then the extracts are combined, washed with sat. sodium chloride solution, dried, and evaporated in vacuo to give 13.1 g (0.0434 moles) of the above titled compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US03984419 |
| Source dataset | uspto-grants-1976_10 |
| ORD ID | ord-c26ec77844bb4ce592a6bd75be35bff4 |
| Source note | uspto-grants-1976_10 |